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The retention of a solute in RP chromatography is a very complex process which depends on many factors. Therefore, the study of the influence of a mobile phase modifier concentration on the retention in different reversed phase chromatographic systems is very important for understanding the rules governing retention and mechanisms of substance separation in a chromatographic process. Composition changes and the nature of mobile phases enable tuning of the separated analytes' retention over a wide range of retention parameters and optimization of the chromatographic process as well. Optimization of the chromatographic process can be achieved by several different methods; one of them is the so-called interpretative strategy. The key approach adopted in this strategy is the implementation of adequate retention models that couple the retention of solute with the composition of a mixed mobile phase. The use of chemically bonded stationary phases composed of partially non-bonded silica matrix and organic ligands bonded to its surface in everyday chromatography practice leads to questions of the correct definition of the retention model and the dominant retention mechanism in such chromatographic systems. The retention model for an accurate prediction of retention factor as a function of modifier concentration and the heterogeneity of the adsorbent surface should be taken into consideration. In this work the influence of mobile-phase composition on the retention of sixteen model substances such as phenols, quinolines, and anilines used as test analytes in different RP-TLC systems with CN-, NH2-, and Diol-silica polar bonded stationary phases has been studied. The aim of this study is to compare the performance of three valuable retention models assumed as the partition, adsorption/partition, and adsorption mechanism of retention. All the models were verified for different RP-TLC systems by three statistical criteria. The results of investigations presented in this work demonstrate that the best agreement between the experimental and calculated Rf values was obtained by the use of new-generation retention models, which assume heterogeneity of adsorbent surface. The results reported here show that heterogeneity of the adsorbent surface may be important in analysis of the elution process in liquid chromatography. Consideration of the goodness of fit for the experimental data to the examined retention models is in conformity with the adsorption mechanism of retention on all polar bonded stationary phases in most eluent systems for most investigated compounds.
BACKGROUND: Previous evaluations of HPLC as a tool for detection of hemoglobin variants have done so within newborn-screening programs and/or by use of stored samples. We describe a 32-month prospective study in a clinical diagnostic laboratory in which we evaluated the imprecision of HPLC retention times and determined the retention times for hemoglobin variants seen in a multiethnic setting. METHODS: We analyzed all samples on the Bio-Rad Variant II HPLC system. For normal hemoglobin fractions and hemoglobin variants, we recorded and analyzed their retention times, their proportion of the total hemoglobin (%), and the peak characteristics. We compared the imprecision of retention time with the imprecision of retention time normalized to the retention time of hemoglobin A0 (Hb A0) and to the retention time of Hb A2. Alkaline and acid hemoglobin electrophoresis, and in certain cases globin chain electrophoresis, isoelectric focusing, and DNA analysis, were performed to document the identities of the hemoglobin variants. RESULTS: The mean (SD) imprecision (CV) of the retention time was 1.0 (0.7)% with no statistical difference compared with the imprecision for normalized retention times. Among 60,293 samples tested, we encountered 34 unique hemoglobin variants and 2 tetramers. Eighteen variants and 2 tetramers could be identified solely by retention time and 3 variants by retention time and proportion of total hemoglobin. Four variants could be identified by retention time and peak characteristics and eight variants by retention time and electrophoretic mobility. One variant (Hb New York) was missed on HPLC. Retention time on HPLC was superior to electrophoresis for the differentiation and identification of six members of the Hb J family, four members of the Hb D family, and three variants with electrophoretic mobilities identical or similar to that of Hb C. Six variants with electrophoretic mobilities identical or similar to that of Hb S could be differentiated and identified by retention time and proportion of total hemoglobin. HPLC detected two variants (Hb Ty Gard and Hb Twin Peaks) missed on electrophoresis. CONCLUSIONS: The retention time on HPLC is reliable, reproducible, and in many cases superior to conventional hemoglobin electrophoresis for the detection and identification of hemoglobin variants. Confirmatory testing by electrophoresis can be eliminated in the majority of cases by use of retention time, proportion of total hemoglobin, and peak characteristics of HPLC.
UNLABELLED: There is no consensus on the amount of (131)I for treatment of patients with well-differentiated thyroid carcinoma; usual amounts vary widely. Body retention of (131)I has been shown to be a valuable index of radiation toxicity. If a broad range of body retentions occurs among patients, then high and low retentions will be a basis for modifying the usual prescriptions for (131)I to ensure safety and increase efficacy. METHODS: After withdrawal of thyroid hormone in 87 patients, the fractional retention of diagnostic (131)I in each body was measured at 2 d by a scintillation probe. In 43 patients, the retention was measured 2 d after therapeutic (131)I. RESULTS: Diagnostic retention varied from 0.01 to 0.51, with a median of 0.15. These retentions did not correlate with any index of health, thyroid hormone, or carcinoma status. Seventeen patients, previously treated with (131)I, exhibited a significantly lower mean retention. In 43 patients, retention of diagnostic (131)I was highly correlated with retention of therapeutic (131)I: diagnostic predicted therapeutic retention with a mean error of 0.04. In 10 patients receiving thyroxine, the mean retention of diagnostic (131)I after recombinant human TSH (rhTSH) was strikingly lower, 0.06, with a range of 0.016-0.16. CONCLUSION: Body retentions of (131)I are easily measured and vary considerably among patients. Because increased therapeutic (131)I will impart greater irradiation of tumor, and body retention has been accepted as an index of toxicity from (131)I, the use of body retention could enable prescriptions of therapeutic (131)I that enable increased efficacy while ensuring safety. If tumor retention is not proportionally decreased with the body retention of (131)I after rhTSH, then rhTSH may enable increased therapeutic efficacy.
STATEMENT OF PROBLEM: The elastic property of Ti-Ni alloy may be a desirable property for cast removable partial dentures. However, little is known about the retentive properties of cast Ti-Ni alloy clasps. PURPOSE: This in vitro study investigated the retentive force of various types of clasps during repeated cycles of placement and removal to determine whether Ti-Ni alloy clasps maintain their initial retentive force under varied conditions, including different retentive undercut depths and clasp size (thickness and width). MATERIAL AND METHODS: The test models were developed using a mandibular dentiform with a horizontal plane of occlusion. Two complete metal abutment crowns were made for the left second molar, differing only in retentive undercut depths. A total of 98 clasps (n=7) were fabricated, including 14 wrought wire clasps and 28 clasps from each of the following alloys: Co-Cr alloy (Biosil), Type IV gold alloy (Cast-4), and Ti-Ni alloy (TN-10). Clasps were made to engage one of 2 retentive undercut depths (0.25 mm or 0.75 mm) and were made in 2 sizes (0.8 mm or 1.4 mm). Each clasp was radiographically examined for casting defects and porosity. The force (N) required to remove the clasps was measured using a universal testing machine with a crosshead speed of 10 mm/min. After measuring the retentive force, a masticatory simulator was used to cycle the clasps on and off the metal crown 500 times, simulating the insertion and removal of a removable partial denture clasp. The cycling sequence was repeated 10 times, and retention force was measured after each sequence. The internal surface of the clasp arms was examined for evidence of metal fatigue using scanning electron microscopy. Data were subjected to 2-way and 4-way analysis of variance, followed by Scheffe's multiple comparison test (alpha=.05). RESULTS: Co-Cr alloy and gold alloy clasps in the 0.25-mm retentive undercut groups experienced a gradual decrease in retentive force measurements (P<.001). In contrast, the Ti-Ni alloy clasps maintained a retentive force of approximately 1.8 N and 2.6 N for the 0.8 mm and 1.4 mm clasp groups, respectively. Although Ti-Ni alloy clasps' retentive force was reduced slightly after the first cycling sequence, it was negligible compared with other clasps tested. The wrought wire clasps also retained their retentive force until the final cycling sequence. A similar trend was found in the clasp groups engaging 0.75-mm retentive undercuts. CONCLUSION: Although the end-point retention for all the clasps was similar, there was less change in the retentive force of the cast Ti-Ni alloy clasps after repeated cycling sequences of simulated placement and removal.
PURPOSE: We report how the incidence of primary and recurrent acute urinary retention changed in England between 1998 and 2003. In addition, we present data on changes with time in the use of prostatectomy after acute urinary retention and recurrent acute urinary retention. MATERIALS AND METHODS: Data were extracted from the Hospital Episode Statistics database of the Department of Health in England. Patients were included in the study if an International Classification of Diseases, Tenth Revision code for acute urinary retention or an operative procedure code for transurethral prostate resection was present in any diagnosis or procedure fields of the Hospital Episode Statistics database. A total of 165,527 men were identified to have been hospitalized with acute urinary retention in the study period. RESULTS: The incidence of primary acute urinary retention was 3.06/1,000 men yearly. Acute urinary retention was spontaneous in 65.3% of cases. The incidence of acute urinary retention decreased from 3.17/1,000 men yearly in 1998 to 2.96/1,000 yearly in 2003. Surgical treatment following spontaneous acute urinary retention decreased 20% from 32% in 1998 to 26% in 2003. This trend coincided with a 20% increase in the rate of recurrent acute urinary retention. CONCLUSIONS: The slight decrease in the incidence of primary acute urinary retention suggests that the shift away from surgical treatment for benign prostatic hyperplasia has not resulted in an increase in acute urinary retention. The increase in recurrent acute urinary retention suggests that the observed decrease in surgery after acute urinary retention may have put more men at risk for acute urinary retention recurrence.
UNLABELLED: The aims of this study were: (i) to evaluate and compare retention of two-teeth (implant) supported mandibular overdenture with either stud or magnetic attachments during linear (axial) and rotational (paraxial) dislodgements; (ii) to compare retentive properties before and after wear simulation. The test group consisted of five magnetic and four stud overdenture attachments (n = 12 specimens for each attachment type). Retention in axial direction was evaluated on one-tooth (implant) model by measuring maximum retentive force (N) and range of retention (mm) during the linear dislodgement. Retention in the paraxial direction was evaluated on mandibular-overdenture model by measuring the maximum retentive force (N) during three types of rotational dislodgements - anterior, lateral and posterior. The minimum number of cycles required to simulate wear was determined by special wear test. Afterwards, the wear was simulated in the test group, and retention in axial and paraxial directions was measured again. STATISTICAL ANALYSIS: one-way anova, Scheffe post hoc and paired-samples t-tests (P < 0.05). Initially, studs had higher retention (4-11 N) than magnets (4.5-6 N) in axial direction. After the wear simulation, it had decreased from 76% to 48% for some of the studs and had become similar to the retention of magnetic attachments. Magnets had lower retention range (0.2-0.3 mm) than studs (0.5-1.1 mm). Studs provided similar or higher retention in paraxial directions than magnetic attachments both before and after wear simulation. Retentive properties of magnets decreased mostly with posterior rotational dislodgement. Retentive properties of stud overdenture attachments were less constant.
Masticatory forces cause fatigue to cement-retained crowns and abutments and may adversely effect retention. The relation between the number of load cycles and the retentive forces is important. This study evaluated the effect of compressive cyclic loading on the retentive forces of a temporary cement used to retain implant crowns and the relationship between load cycles and retentive forces. Ten castings and implant abutments were cemented with zinc oxide-eugenol temporary cement. The retentive force necessary to dislodge the casting from the abutment was determined before and after the application of 2 Hz of vertical off-axis 3-mm sinusoidal-type compressive cyclic loading between 20 and 130 N for 500000, 1000000, and 5000000 cycles. These forces were equivalent to approximately 6 months, 1 year, and 5 years of human mastication. Data before and after the applied loading were analyzed with a paired sample t test (alpha = 0.05). The retentive forces of the 3 groups were analyzed by 1-way analysis of variance and post hoc by Scheffé multiple comparison (alpha = 0.05). The relation of the loading and the altered retentive forces were analyzed with the Pearson correlation coefficient. Compressive cyclic loading reduced the retentive forces significantly in all groups (P = .000). The retentive forces were reduced 16.75%, 18.73%, and 19.68% during the applied loading cycles of 500000, 1000000, and 5000000. All reduced retentive forces were not significantly different (P = .792). Although cyclic loading reduced the retentive forces, the increased cycles had little relationship (R = 0.119) to the decreased retentive forces of the temporary cement. The relationship between occlusal loading and retentive force can influence the choice of a temporary cement for a particular clinical situation.
The chromatographic identity of a compound can be determined by four parameters, namely, I, A, Z and (GRF). These are interrelated in a linear regression equation, given in the paper as Eq. 8. The retrieval of structural information from retention data requires the introduction of a new meaning to the Kováts retention index, the use of column difference (delta I) to characterize functional groups, the redefinition of the role of electronegative oxygen and nitrogen atoms, and the division of retention index (I) into contributions from atoms and from functional groups. The separation of retention index (I) into molecular and interaction contributions is a necessary condition for retention index prediction from structure and also for structure information retrieval from retention data. According to Eq. 8 the retention index is uniquely determined by three parameters, namely A, Z and (GRF). For prediction of retention index, the A value is assigned a value of 100 index units (i.u.), the Z value is obtained directly from the compound, and the (GRF) value is pre-calibrated. In Eq. 10, the m and n values represent the pre-calibrated terms for a quantitative structure-retention index relationship. These terms account for the positive and negative retention contributions from polar and polarizable atom groups. All atom groups that are different from methylene and methyl groups will interact with the stationary phase and contribute to retention. The m and n values for various functional, polar and polarizable atom groups and their column differences (delta I values) are the results of interactions between the solute and the stationary phase and are structure dependent. The interaction increases with increasing polarities of the solute and the stationary phase. The column difference not only reflects the strength of the interaction, but is also characteristic of the functional and polarizable groups. The retrieval of structural information from retention data is equivalent to obtaining Z and (GRF) values from known I and delta I values, which is straightforward for monofunctional compounds. For multi-functional compounds, additional data will be needed for retrieval of structural information. These can be obtained from derivatization of the unknown compound, from its chemical reactions with other reagents, from GC-MS analysis and from structure match using internal or external standards. The additional data required will depend upon the complexity of the unknown structure. This approach demonstrates that a system can be devised to utilize GC retention characteristics uniquely for structure elucidation.
A rapid retention time alignment algorithm was developed as a preprocessing utility to be used prior to chemometric analysis of large datasets of diesel fuel profiles obtained using gas chromatography (GC). Retention time variation from chromatogram-to-chromatogram has been a significant impediment against the use of chemometric techniques in the analysis of chromatographic data due to the inability of current chemometric techniques to correctly model information that shifts from variable to variable within a dataset. The alignment algorithm developed is shown to increase the efficacy of pattern recognition methods applied to diesel fuel chromatograms by retaining chemical selectivity while reducing chromatogram-to-chromatogram retention time variations and to do so on a time scale that makes analysis of large sets of chromatographic data practical. Two sets of diesel fuel gas chromatograms were studied using the novel alignment algorithm followed by principal component analysis (PCA). In the first study, retention times for corresponding chromatographic peaks in 60 chromatograms varied by as much as 300 ms between chromatograms before alignment. In the second study of 42 chromatograms, the retention time shifting exhibited was on the order of 10 s between corresponding chromatographic peaks, and required a coarse retention time correction prior to alignment with the algorithm. In both cases, an increase in retention time precision afforded by the algorithm was clearly visible in plots of overlaid chromatograms before and then after applying the retention time alignment algorithm. Using the alignment algorithm, the standard deviation for corresponding peak retention times following alignment was 17 ms throughout a given chromatogram, corresponding to a relative standard deviation of 0.003% at an average retention time of 8 min. This level of retention time precision is a 5-fold improvement over the retention time precision initially provided by a state-of-the-art GC instrument equipped with electronic pressure control and was critical to the performance of the chemometric analysis. This increase in retention time precision does not come at the expense of chemical selectivity, since the PCA results suggest that essentially all of the chemical selectivity is preserved. Cluster resolution between dissimilar groups of diesel fuel chromatograms in a two-dimensional scores space generated with PCA is shown to substantially increase after alignment. The alignment method is robust against missing or extra peaks relative to a target chromatogram used in the alignment, and operates at high speed, requiring roughly 1 s of computation time per GC chromatogram.